Continuous extraction device and extraction method

By designing a continuous extraction device, continuous circulation extraction is achieved by using heating distillation and liquid level elevation difference, which solves the problem of low efficiency of traditional methods, significantly improves extraction efficiency and saves costs.

CN110772831BActive Publication Date: 2025-02-11BEIJING RED AVENUE INNOVA +1
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN201911129046.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2019-11-18
Publication Date
2025-02-11
Estimated Expiration
2039-11-18

AI Technical Summary

Technical Problem

The traditional Soxhlet extraction and physical soaking methods are inefficient when extracting and filling oil rubber, requiring a large amount of solvent and time, which cannot meet the needs of large-scale rubber refining formulas.

Method used

A continuous extraction device is designed, including a heating device and a multi-stage extraction tank connected in series through pipelines, and continuous circulation extraction is achieved through heating distillation and liquid level elevation difference.

Benefits of technology

It significantly improves the extraction work efficiency, shortens time, saves solvent and labor costs, and can effectively extract a variety of difficult-to-extract materials.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN110772831B_ABST
    Figure CN110772831B_ABST
Patent Text Reader

Abstract

The present invention relates to the technical field of chemical equipment, and in particular to a continuous extraction device and an extraction method using the continuous extraction device. The continuous extraction device comprises a heating device and a plurality of extraction tanks connected in series through pipelines, wherein the heating device is used to heat the first-stage extraction tank, and starting from the second-stage extraction tank, the liquid outlet of the first-stage extraction tank is higher than the liquid outlet of the next-stage extraction tank, and the liquid outlet of the last-stage extraction tank is higher than the liquid outlet of the first-stage extraction tank, and a solvent addition port is arranged on the top of the first-stage extraction tank. The multi-stage extraction tank realizes continuous cyclic extraction through heating distillation and the elevation difference of the liquid level in each stage of the extraction tank, and has a simple structure and operation, and can greatly improve the working efficiency of the extraction process.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to the technical field of chemical equipment, and in particular to a continuous extraction device and an extraction method using the continuous extraction device. Background Art

[0002] In the field of rubber and tires, specific types of rubber compounds are often used for formula design, testing, etc., such as various types of natural rubber, styrene-butadiene rubber, butadiene rubber, chloroprene rubber, etc. Sometimes it is necessary to verify the performance of compounds with different oil filling amounts, and there is no relevant brand of rubber on the market, so it is necessary to extract the oil filling in the rubber by yourself. Traditional Soxhlet extraction and fat extraction equipment can only perform a small amount of multiple operations, and each rubber refining formula requires several kilograms of rubber, which is far from being satisfied. Usually, experimental personnel in this field also use the method of physical immersion. First, the block rubber is cut into thin sheets, and then placed in a larger container to add a suitable organic solvent that does not destroy the rubber structure, soak at room temperature, and change the solvent every other day or several days until the extraction standard is reached. Since the oil and rubber in the oil-filled rubber are mixed very fully, the extraction speed is extremely slow at room temperature, so this method requires a large-capacity container and a large amount of solvent for intermittent replacement, which is inefficient and usually takes several weeks to complete, which inevitably consumes a lot of manpower, material and time costs. Summary of the invention

[0003] In order to solve the above technical problems, the present application provides a continuous extraction device and an extraction method using the continuous extraction device, in order to achieve the purpose of improving the extraction work efficiency.

[0004] In order to achieve the above-mentioned purpose, according to one aspect of the present technical solution, the present technical solution provides a continuous extraction device.

[0005] According to the continuous extraction device of the embodiment of the present application, it includes a heating device and multiple extraction tanks connected in series by pipelines, the heating device is used to heat the first-stage extraction tank, starting from the second-stage extraction tank, the liquid outlet of the previous-stage extraction tank is higher than the liquid outlet of the next-stage extraction tank, the liquid outlet of the last-stage extraction tank is higher than the liquid outlet of the first-stage extraction tank, and a solvent addition port is provided on the top of the first-stage extraction tank.

[0006] Furthermore, the first-stage extraction tank and the second-stage extraction tank are connected via a distillation pipeline, and one end of the distillation pipeline is arranged on the top of the first-stage extraction tank.

[0007] Furthermore, the end of the pipeline between two adjacent extraction tanks leads to the bottom of the extraction tank.

[0008] Furthermore, the extraction tank and the pipeline form a closed thermal insulation system.

[0009] Furthermore, a flow control valve is provided on the pipeline between two adjacent extraction tanks.

[0010] Furthermore, the volumes of the extraction tanks at each stage are the same or different.

[0011] In order to achieve the above-mentioned purpose, according to the second aspect of the present technical solution, the present technical solution also provides an extraction method using the above-mentioned continuous extraction device provided by the present invention.

[0012] According to the extraction method of the embodiment of the present application, it includes:

[0013] Add the material to be extracted into each level of extraction tanks. The upper edge of the material should not be higher than the liquid outlet. Add the solvent into the first level extraction tank.

[0014] Turn on the heating device to heat the first-stage extraction tank to make the solvent in a distillation state. The solvent flows through each stage of extraction tanks in turn and then flows back to the first-stage extraction tank, and the cycle continues;

[0015] During the extraction process, add solvent when the liquid level in the first-stage extraction tank drops.

[0016] Further, the solvent in the first stage extraction tank is maintained in a distillation state for extraction for 0.5-50 hours.

[0017] Furthermore, the solvent is selected from at least one of toluene, xylene, ethanol, ethyl acetate, acetone, methanol, cyclohexane, petroleum ether, chloroform, and tetrahydrofuran.

[0018] Furthermore, the materials to be extracted include rubber, Chinese medicinal materials, nuts and spices.

[0019] The continuous extraction device and extraction method provided by the present invention realize continuous cyclic extraction through multi-stage extraction tanks, heating distillation and the elevation difference of the liquid levels in the extraction tanks at each stage. The structure and operation are simple and the working efficiency of the extraction process can be greatly improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The drawings constituting a part of this application are used to provide a further understanding of this application, so that other features, purposes and advantages of this application become more obvious. The schematic embodiment drawings and their descriptions of this application are used to explain this application and do not constitute an improper limitation on this application. In the drawings:

[0021] Figure 1 A schematic diagram of the structure of a continuous extraction device provided in an embodiment of the present application is shown schematically;

[0022] Figure 2 A schematic diagram of the structure of another continuous extraction device provided in an embodiment of the present application is shown; and

[0023] Figure 3 A schematic structural diagram of another continuous extraction device provided in an embodiment of the present application is given schematically. DETAILED DESCRIPTION

[0024] In order to enable those skilled in the art to better understand the solution of the present application, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present application.

[0025] It should be noted that the terms "first", "second", etc. in the specification and claims of the present application and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequential order. It should be understood that the data used in this way can be interchanged where appropriate, so that the embodiments of the present application described here. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions, for example, a process, method, system, product or device comprising a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or devices.

[0026] In the present application, the directions or positional relationships indicated by the terms "upper", "lower", "inner", "middle", "outer", "front", "back", etc. are based on the directions or positional relationships shown in the drawings. These terms are mainly used to better describe the present application and its embodiments, and are not used to limit the indicated devices, elements or components to have a specific direction, or to be constructed and operated in a specific direction.

[0027] In addition, some of the above terms may be used to express other meanings in addition to indicating orientation or positional relationship. For example, the term "on" may also be used to express a certain dependency or connection relationship in some cases. For those of ordinary skill in the art, the specific meanings of these terms in this application can be understood according to specific circumstances.

[0028] In addition, the terms "disposed", "connected", and "fixed" should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral structure; it can be a mechanical connection, or an electrical connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be an internal connection between two devices, elements, or components. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0029] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. Figure 1-3 The present application is described in detail with reference to embodiments.

[0030] like Figure 1-3 As shown, the continuous extraction device includes a heating device 1 and a plurality of extraction tanks connected in series through a pipeline 2. The heating device 1 is used to heat the first-stage extraction tank 3-1. Starting from the second-stage extraction tank 3-2, the liquid outlet of the previous-stage extraction tank is higher than the liquid outlet 301 of the next-stage extraction tank, and the liquid outlet of the last-stage extraction tank is higher than the liquid outlet of the first-stage extraction tank 3-1. The top of the first-stage extraction tank 3-1 is provided with a solvent addition port 302. As shown in the figure, the first-stage extraction tank 3-1 and the second-stage extraction tank 3-2 are connected by a distillation pipeline, one end of the distillation pipeline is arranged at the top of the first-stage extraction tank 3-1, and the distillation pipeline is arranged in an n-shaped shape. The solvent vapor generated after distillation continuously enters the second-stage extraction tank 3-2 through the n-shaped distillation pipeline. The heating device can be various conventional devices for heating materials in the art, including but not limited to heating sleeves, heating furnaces, heating belts, etc. The specific heating principle can be resistance heating or electromagnetic heating. Those skilled in the art can make specific choices according to needs, and this application does not make too many restrictions.

[0031] When the continuous extraction device in this embodiment is used, first, the material to be extracted is added to each stage of the extraction tank. In order to improve the extraction effect, it is best to cut the material 5 into small pieces or slices, and add the solvent to the first stage extraction tank 3-1. It is best to make the upper edge of the material 5 not higher than the liquid outlet 301 to ensure that the material can be fully immersed in the solvent and fully extracted; then the heating device 1 is turned on to heat the first stage extraction tank 3-1 to make the solvent inside it in a distillation state. The solvent distilled out of the first stage extraction tank 3-1 will enter the second stage extraction tank 3-2, and the solvent liquid level in the second stage extraction tank 3-2 will gradually rise. When the liquid level reaches the position of the liquid outlet 301 of the second stage extraction tank 3-2, the solvent liquid level in the second stage extraction tank 3-2 will flow out through the pipeline into the next extraction tank. In this way, the solvent distilled out of the first stage extraction tank 3-1 will flow through the extraction tanks of each stage in turn and finally flow back to the first stage extraction tank 3-1, and the cycle is repeated. During the extraction process, after the liquid level of the first extraction tank 3-1 drops, the solvent needs to be added in time through the solvent adding port 302 to keep the liquid level in the first extraction tank 3-1 within a certain height range. The liquid level in the extraction tank can be observed by a liquid level gauge or an observation window set on the tank body. The specific implementation method can refer to the existing technology and will not be repeated here.

[0032] In the above embodiment, the material to be extracted and the solvent contained in the extraction tank are extracted under the state of heating and distillation on the one hand, and the solvent circulates in the continuous extraction device and the solvent and the material move relative to each other through the distillation operation and the height difference between the extraction tanks at each level. The above two aspects increase the speed at which the extracted phase in the material enters the solvent, improve work efficiency, and save time and labor costs.

[0033] The continuous extraction device in this embodiment can be applied to a variety of materials that are difficult to extract, including but not limited to rubber. In the extraction operation, the specific extraction time can be specifically selected according to the different materials and solvents. For example, when extracting oil-containing rubber, it is preferred to keep the solvent in the first-stage extraction tank in a distillation state for 0.5-50 hours. In addition, in addition to being applied to rubber extraction, the continuous extraction device and extraction method of the present invention can also be applied to extraction in other fields, such as chemical, food, Chinese medicinal materials, spices and other industries.

[0034] The solvent used for extraction can be various commonly used organic solvents for extraction, including but not limited to at least one of toluene, xylene, ethanol, ethyl acetate, acetone, methanol, cyclohexane, petroleum ether, chloroform and tetrahydrofuran. The selected solvent needs to have a good extraction effect on the phase to be extracted on the one hand, and on the other hand, it must ensure that the damage to the material structure is reduced. For example, for rubber materials, a good solvent can be at least one of toluene, ethanol, and ethyl acetate. During the extraction process, the mass ratio of the added material to the solvent can be 1:1.2 to 1:1.8, preferably 1:1.2 to 1:1.5.

[0035] In some embodiments, Figure 1-3 As shown, the end of the pipe between two adjacent extraction tanks is passed into the lower part of the extraction tank, so that the solvent can enter from the lower part of the extraction tank and flow out from the upper liquid outlet 301, further strengthening the relative movement between the solvent and the material and improving the extraction efficiency. Optionally, referring to the pipe inserted into the second-stage extraction tank in the attached figure, the pipe 2 is inserted into the tank body from the top of the extraction tank, so that the end is located in the extraction tank near the bottom of the tank; Optionally, referring to the pipe connecting the last-stage extraction tank with the first-stage extraction tank 3-1 in the attached figure, the pipe is directly connected to the lower part of the extraction tank from the outside of the tank body, so that the space occupied by the pipe 2 inside the extraction tank can be reduced.

[0036] Preferably, the extraction tank of the extraction device in the embodiment forms a closed heat preservation system with the pipeline 2 to reduce heat loss. In addition, all equipment in the extraction device meets the requirements of high temperature and high pressure resistance.

[0037] like Figure 1-3As shown, a flow control valve 4 is provided on the pipeline 2 between two adjacent extraction tanks. During the extraction process, the flow control valve 4 can be adjusted to adjust the solvent flow in the pipeline 2 to prevent the solvent from flowing too fast or too slow locally.

[0038] Preferably, each level of extraction tanks is configured to be detachably connected to facilitate the addition of materials and the assembly of the extraction device; except for the first-level extraction tank 3-1, the remaining levels of extraction tanks can also be preset with solvent addition ports 302, and solvent can be added through the solvent addition ports 302 according to the needs of the specific extraction process.

[0039] It should be noted that the size of the extraction tank in the embodiment of the present application can be specifically set according to the type of material, operating environment and process requirements, and the volumes of the extraction tanks at each level can be the same or different.

[0040] The extraction device according to the above embodiment may also include other necessary components or structures, for example, a valve for releasing the solvent needs to be provided at the bottom of the extraction tank, and a pressure gauge, a temperature sensor and a liquid level gauge for monitoring the extraction process parameters need to be provided, and the corresponding layout positions and connection relationships can refer to the chemical equipment in the prior art. The connection relationship, operation and working principle of each unmentioned structure are known to ordinary technicians in this field and will not be described in detail here.

[0041] The present invention is further described below in conjunction with specific examples. However, the present invention is not limited by these examples. The sources of the raw materials and reagents in each example are shown in the following table.

[0042] Table 1 Sources of raw materials and reagents

[0043] Raw material name source SBR1712 styrene butadiene rubber (37.5% oil-extended) Lanzhou Petrochemical Company SBS4452 oil glue (33% oil extended) Yanshan Petrochemical Company SBR1712 styrene butadiene rubber (37.5% oil-extended) Qilu Petrochemical Anhydrous ethanol Sinopharm Group Toluene Sinopharm Group Ethyl acetate Sinopharm Group Cashew Shell Qingdao Guangrui Fruit Company Methanol Sinopharm Group Petroleum ether Sinopharm Group

[0044] Example 1

[0045] The continuous extraction device used in this embodiment is as follows Figure 1As shown, it includes two extraction tanks, namely the first-stage extraction tank 3-1 and the second-stage extraction tank 3-2, and the effective volume of the two extraction tanks is 7L. 5kg of SBR1712 styrene-butadiene rubber produced by Lanzhou Petrochemical Company is cut into sheet-shaped rubber blocks of about 20cm×20cm×0.5cm, and added to two series-connected high-temperature and high-pressure extraction tanks with an effective volume of 7L each. The rubber sheet is fixed so that its height is not higher than the position of the liquid outlet, and the storage tank is kept in a closed state. 3kg of toluene solvent is added to the first-stage extraction tank 3-1, and the heating device 1 at the bottom is turned on to heat the toluene in the first-stage extraction tank 3-1 to be in a distillation state. The solvent level is observed, and when the liquid level drops, toluene is added through the solvent addition port 302 on the first-stage extraction tank 3-1, and the toluene in the second-stage storage tank 3-2 flows back to the first-stage extraction tank 3-1 through the liquid outlet to complete the cycle. The distillation state is maintained for 24 hours, and the extraction is completed. The mass of the solvent added through the solvent addition port 302 is 3kg. After releasing the solvent, the extracted SBR1712 rubber was taken out, dried in an oven at 60°C to constant weight, and weighed. The weight of the remaining rubber was 3.20 kg, the oil extraction mass fraction was 36.5%, and the extraction rate was 96%.

[0046] Example 2

[0047] The continuous extraction device used in this embodiment is as follows Figure 2 As shown, it includes three extraction tanks, namely the first-stage extraction tank 3-1, the second-stage extraction tank 3-2 and the third-stage extraction tank 3-3. The effective volume of the three extraction tanks is 7L. 8kg of SBS4452 oil glue produced by Yanshan Petrochemical Company is cut into sheet-shaped rubber blocks of about 20cm×20cm×0.5cm, and added evenly into three series-connected high-temperature and high-pressure resistant extraction tanks with an effective volume of 7L. The rubber sheets are fixed so that their height is not higher than the position of the liquid outlet to keep the extraction tanks airtight. state, add 3kg of ethanol solvent to the first-stage extraction tank 3-1, turn on the heating device 1 at the bottom, heat to make ethanol in a distillation state, and when the liquid level in the first-stage extraction tank 3-1 drops, add ethanol through the solvent addition port 302 of the first-stage extraction tank 3-1, and the ethanol in the second-stage extraction tank 3-2 flows back to the third-stage extraction tank 3-3 through the liquid outlet 301, and the ethanol in the third-stage extraction tank 3-3 flows back to the first-stage extraction tank 3-1 through the liquid outlet 301, completing the cycle. Keep the distillation state for 30 hours, and the extraction is completed. The mass of the solvent ethanol added during the extraction process is 9kg. Release the solvent, take out the extracted SBS 4452 oil-based rubber compound, dry it in an oven at 60°C to constant weight, weigh it, and the weight of the remaining rubber compound is 5.50kg, the oil extraction mass fraction is 31.2%, and the extraction rate is 93.7%.

[0048] Example 3

[0049] The continuous extraction device used in this embodiment is as follows Figure 3As shown, it includes four extraction tanks, namely, a first-stage extraction tank 3-1, a second-stage extraction tank 3-2, a third-stage extraction tank 3-3 and a fourth-stage extraction tank 3-4. The effective volumes of the four extraction tanks are 7L, 6L, 6L and 5L respectively. 10kg of SBR1712 styrene-butadiene rubber produced by Qilu Petrochemical Company is cut into sheet-like rubber blocks of about 20cm×20cm×0.5cm, and added to four series-connected high-temperature and high-pressure resistant extraction tanks. The rubber sheets are fixed so that their height is not higher than the position of the liquid outlet 301, and the extraction tanks are kept in a closed state. 3kg of ethyl acetate solvent is added to tank 3-1, and the heating device 1 at the bottom is turned on to heat the ethyl acetate to make it in a distillation state. When the liquid level drops, ethyl acetate is added through the solvent addition port 302 of the first-stage extraction tank 3-1. The ethyl acetate in the second-stage extraction tank 3-2 flows back to the third-stage extraction tank 3-3 through the liquid outlet 301, and the ethyl acetate in the third-stage extraction tank 3-3 flows back to the fourth-stage extraction tank 3-4 through the liquid outlet 301. The ethyl acetate in the fourth-stage extraction tank 3-4 flows back to the first-stage extraction tank 3-1 through the liquid outlet 301, completing the cycle. The distillation state is maintained for 36 hours, and the extraction is completed. The mass of the solvent added during the extraction process is 10kg. The solvent is released, and the extracted SBR1712 rubber material is taken out, dried in an oven at 40°C to constant weight, and weighed. The weight of the remaining rubber material is 6.6kg, the oil extraction mass is 34%, and the extraction rate is 90.7%.

[0050] Comparative Example 1

[0051] 5kg of SBR1712 styrene-butadiene rubber produced by Lanzhou Petrochemical Company was cut into 20cm×20cm×0.5cm pieces, added to a 15L storage tank, and 8kg of toluene solvent was added. After soaking at room temperature for 48h, the toluene solvent was replaced, and the extraction was continued for 48h. The solvent was replaced again for 5 times. The solvent was released, the extracted SBR1712 rubber was taken out, and dried in an oven at 60℃ to constant weight. The remaining rubber weight was 3.95kg, the oil extraction mass was 21%, and the extraction rate was 56%.

[0052] Comparative Example 2

[0053] 8kg of SBS4452 oil rubber produced by Yanshan Petrochemical Company was cut into 20cm×20cm×0.5cm pieces, added to a 30L storage tank, and 14kg of ethanol solvent was added. After soaking at room temperature for 48h, the ethanol solvent was replaced, and the extraction was continued for 48h. The solvent was replaced again for 7 times. The solvent was released, the extracted SBS4452 rubber was taken out, dried in an oven at 60℃ to constant weight, and weighed. The remaining rubber weight was 6.416kg, the oil extraction mass was 19.8%, and the extraction rate was 60%.

[0054] Comparative Example 3

[0055] 10kg of SBR1712 styrene-butadiene rubber produced by Qilu Petrochemical Company was cut into 20cm×20cm×0.5cm pieces, added evenly to a 40L storage tank, and 18kg of ethyl acetate solvent was added. After soaking at room temperature for 48h, the ethyl acetate solvent was replaced, and the extraction was continued for 48h. The solvent was then replaced 5 times. The solvent was released, the extracted SBR1712 rubber was taken out, dried in an oven at 40℃ to constant weight, and weighed. The weight of the remaining rubber was 8.3kg, the oil extraction mass was 17%, and the extraction rate was 45%.

[0056] It can be seen from the comparative examples that conventional extraction not only consumes a huge amount of solvent and takes a long time, but also has a poor extraction effect and is very inefficient, which is far inferior to the extraction effect of Examples 1-3 of the present application.

[0057] Example 4 Extraction of Cashew Oil from Cashew Nut Shells

[0058] The continuous extraction device used in this embodiment is as follows Figure 2 As shown, it includes three extraction tanks, namely, a first-stage extraction tank 3-1, a second-stage extraction tank 3-2 and a third-stage extraction tank 3-3, each of which has an effective volume of 10 L. 10 kg of cashew nut shells are evenly added to three series-connected high-temperature and high-pressure resistant extraction tanks each having an effective volume of 10 L. The cashew nut shells are fixed so that their height is not higher than the position of the liquid outlet, and the extraction tanks are kept in a closed state. 5 kg of ethanol solvent is added to the first-stage extraction tank 3-1, and the heating device 1 at the bottom is turned on to heat the ethanol to make it in a distillation state. When the liquid level in the first-stage extraction tank 3-1 drops, ethanol is added through the solvent addition port 302 of the first-stage extraction tank 3-1, and the ethanol in the second-stage extraction tank 3-2 flows back to the third-stage extraction tank 3-3 through the liquid outlet 301, and the ethanol in the third-stage extraction tank 3-3 flows back to the first-stage extraction tank 3-1 through the liquid outlet 301, completing the cycle. The distillation state was maintained for 1 hour, and the extraction was completed. The mass of the solvent ethanol added during the extraction process was 13 kg. The solvent containing the extracted phase was released, and the ethanol was distilled to obtain 1.1 kg of cashew nut shell oil. The oil yield of the cashew nut shell was 11%.

[0059] Example 5 Extraction of turpentine from pine needles

[0060] The continuous extraction device used is Figure 2As shown, it includes three extraction tanks, namely the first-stage extraction tank 3-1, the second-stage extraction tank 3-2 and the third-stage extraction tank 3-3. The effective volume of the three extraction tanks is 10L. 10kg of pine needles are evenly added to the three series-connected high-temperature and high-pressure extraction tanks with an effective volume of 10L each. The pine needles are fixed so that their height is not higher than the position of the liquid outlet, and the extraction tanks are kept in a closed state. 5kg of petroleum ether solvent is added to the first-stage extraction tank 3-1, and the heating device 1 at the bottom is turned on to heat the petroleum ether to make it in a distillation state. When the liquid level in the first-stage extraction tank 3-1 drops, petroleum ether is added through the solvent addition port 302 of the first-stage extraction tank 3-1, and the petroleum ether in the second-stage extraction tank 3-2 flows back to the third-stage extraction tank 3-3 through the liquid outlet 301, and the petroleum ether in the third-stage extraction tank 3-3 flows back to the first-stage extraction tank 3-1 through the liquid outlet 301, completing the cycle. The distillation state was maintained for 1.5 hours, and the extraction was completed. The mass of the solvent petroleum ether added during the extraction process was 10 kg. The solvent containing the extracted phase was released, and the petroleum ether was distilled out to obtain 0.19 kg of turpentine oil. The oil yield of pine needles was 1.9%.

[0061] Example 6 Extraction of proanthocyanidins from grape seeds

[0062] The continuous extraction device used in this embodiment is as follows Figure 1 As shown, it includes two extraction tanks, namely the first-stage extraction tank 3-1 and the second-stage extraction tank 3-2. The effective volume of the two extraction tanks is 10L. 8kg of grape seeds are crushed by a crusher and added to two high-temperature and high-pressure extraction tanks with an effective volume of 10L in series. The grape seeds are placed so that their height is not higher than the position of the liquid outlet. The storage tank is kept in a closed state. 4kg of methanol solvent is added to the first-stage extraction tank 3-1. The heating device 1 at the bottom is turned on to heat the methanol in the first-stage extraction tank 3-1 to be in a distillation state. The solvent level is observed. When the liquid level drops, methanol is added through the solvent addition port 302 on the first-stage extraction tank 3-1. The methanol in the second-stage storage tank 3-2 flows back to the first-stage extraction tank 3-1 through the liquid outlet to complete the cycle. The distillation state is maintained for 5h, and the extraction is completed. The mass of the solvent added through the solvent addition port 302 is 8kg. After releasing the solvent containing the extracted phase, the methanol is distilled to obtain a grape seed extract containing proanthocyanidins.

[0063] Some embodiments in this specification are described in a progressive or parallel manner. Each embodiment focuses on the differences from other embodiments, and the same or similar parts between the embodiments can be referenced to each other.

[0064] The above is only a specific embodiment of the present invention, so that those skilled in the art can understand or implement the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but will conform to the widest range consistent with the principles and novel features applied herein.

Claims

1. A continuous extraction device, characterized in that: It comprises a heating device (1) and a plurality of extraction tanks connected in series via a pipeline (2), wherein the heating device (1) is used to heat a first-stage extraction tank (3-1), and starting from a second-stage extraction tank (3-2), the liquid outlet of the first-stage extraction tank is higher than the liquid outlet (301) of the next-stage extraction tank, and the liquid outlet of the last-stage extraction tank is higher than the liquid outlet of the first-stage extraction tank (3-1), and a solvent addition port (302) is provided on the top of the first-stage extraction tank (3-1); The volumes of extraction tanks at each level are the same or different; The first-stage extraction tank (3-1) and the second-stage extraction tank (3-2) are connected via a distillation pipeline, one end of which is arranged on the top of the first-stage extraction tank (3-1).

2. The continuous extraction device according to claim 1, characterized in that: The end of the pipeline between two adjacent extraction tanks leads to the lower part of the extraction tank.

3. The continuous extraction device according to claim 1, characterized in that: The extraction tank and the pipeline (2) form a closed thermal insulation system.

4. The continuous extraction device according to claim 3, characterized in that: A flow control valve (4) is provided on the pipeline (2) between two adjacent extraction tanks.

5. An extraction method using the continuous extraction device according to any one of claims 1 to 4, characterized in that: The extraction method comprises: Add the material to be extracted into each level of extraction tanks. The upper edge of the material should not be higher than the liquid outlet. Add the solvent into the first level extraction tank. Turn on the heating device to heat the first-stage extraction tank to make the solvent in a distillation state. The solvent flows through the extraction tanks of each stage in sequence through the pipeline and then flows back to the first-stage extraction tank, and the cycle continues; During the extraction process, add solvent when the liquid level in the first-stage extraction tank drops.

6. The extraction method according to claim 5, characterized in that Keep the solvent in the first-stage extraction tank in a distillation state for extraction for 0.5-50 hours.

7. The extraction method according to claim 5, characterized in that The solvent is selected from at least one of toluene, xylene, ethanol, ethyl acetate, acetone, methanol, cyclohexane, petroleum ether, chloroform and tetrahydrofuran.

8. The extraction method according to claim 5, characterized in that The materials to be extracted include rubber, Chinese medicinal materials, nuts and spices.

Citation Information

Patent Citations

  • Multi-stage extractor for separating oil from water in solid

    CN103405943A

  • Continuous extraction device

    CN211486621U